Ammonium formate → 4-(1-Acetylpiperidin-4-yl)furo[3,2-c]pyridine

HRID 1018987ノート

反応式

HRID 1018987 の反応式
[C:1]([N:4]1[CH2:9][CH:8]=[C:7]([C:10]2[C:15]3[CH:16]=[CH:17][O:18][C:14]=3[CH:13]=[CH:12][N:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].C([O-])=O.[NH4+]>CO.[Pd]>[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([C:10]2[C:15]3[CH:16]=[CH:17][O:18][C:14]=3[CH:13]=[CH:12][N:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

参加物

5

反応物 2

HCID 2723923Ammonium formate2 回HCID 183997764-(1-Acetyl-1,2,3,6-tetrahydropyridin-4-yl)furo[3,2-c]pyridine

生成物 1

HCID 183997294-(1-Acetylpiperidin-4-yl)furo[3,2-c]pyridine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒2 回HCID 887Methanol溶媒

実験手順

0.7 g of Pd/C (10%) is added to a solution of 3.4 g of the product obtained in Step C and 4.4 g of ammonium formate in 150 ml of anhydrous methanol under a stream of argon. After refluxing for 45 minutes, the reaction mixture is cooled, 4.4 g of ammonium formate and 0.2 g of Pd/C (10%) are added, and the reaction mixture is then heated at reflux for 30 minutes. After returning to ambient temperature, filtration over Celite and concentration under reduced pressure, the residue is taken up in water and then extracted with dichloromethane. The expected product is isolated by extraction, drying, filtration and concentration under reduced pressure.

後処理

  1. temperatureAfter refluxing for 45 minutes
  2. temperaturethe reaction mixture is cooled
  3. temperaturethe reaction mixture is then heated
  4. temperatureat reflux for 30 minutes
  5. customAfter returning to ambient temperature
  6. filtrationfiltration
  7. concentrationover Celite and concentration under reduced pressure
  8. extractionextracted with dichloromethane

出典と根拠

ORDレコード
ord-b0a5f0e040c14630a5e0b2bf9cefc1c3
出典データセット
uspto-grants-2002_11
特許番号
US06486171B2

反応ノート

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